The Department of Chemistry at Princeton University requests funds from the National Center for Research Resources (NCRR) for the purpose of an integrated upgrade of the NMR instrumentation facility, with the focus on biomolecular and bioanalytical applications. The centerpiece for this integrated upgrade is a new 400 MHz NMR spectrometer, which will replace an outdated machine and remove the bottleneck of routine and semi-routine applications. At the same time this enhancement will allow more efficient use of the existing high-field spectrometers for demanding biomolecular research. Additional items of the integrated upgrade will extend the capacity of these high-field instruments. They will open new research opportunities and serve critical research needs primarily in the field of structure, characterization, and dynamics studies of biomolecules. These units are: a complete LC-NMR accessory kit, a slow-spinning high- resolution MAS probehead, a 13C-15N detection optimized triple resonance probehead and a modern computer for efficient off-line data analysis and structure calculations. This upgrade is critical to the success of the research projects in the Department, specifically those of the core user group of eleven faculty members. When implemented, this integrated upgrade of the NMR instrumentation facility will have greatly expanded our total capabilities and increased the efficiency of the highest field NMR spectrometers and associated units, critical for biostructural studies , for a modest total investment.